Journal of Soils and Sediments

, Volume 5, Issue 3, pp 171-181

First online:

Bioassay-directed Fractionation of Organic Extracts of Marine Surface Sediments from the North and Baltic Sea - Part I: Determination and identification of organic pollutants (15 pp)

  • Scarlett BiselliAffiliated withScarlett Biselli Eurofins Wiertz-Eggert-Jörissen Stenzelring 14b 21107 Hamburg DEUTSCHLAND
  • , Ninja ReinekeAffiliated withNinja Reineke Institute of Organic Chemistry University of Hamburg Martin-Luther-King-Platz 6 20146 Hamburg DEUTSCHLAND
  • , Nicolas HeinzelAffiliated withNicolas Heinzel Institute of Organic Chemistry University of Hamburg Martin-Luther-King-Platz 6 20146 Hamburg DEUTSCHLAND
  • , Ulrike KammannAffiliated withDr. Ulrike Kammann Bundesforschungsanstalt für Fischerei Institut für Fischereiökologie Palmaille 9 22767 Hamburg DEUTSCHLAND Email author 
  • , Stephan FrankeAffiliated withStephan Franke Institute of Organic Chemistry University of Hamburg Martin-Luther-King-Platz 6 20146 Hamburg DEUTSCHLAND
  • , Heinrich HühnerfussAffiliated withHeinrich Hühnerfuss Institute of Organic Chemistry University of Hamburg Martin-Luther-King-Platz 6 20146 Hamburg DEUTSCHLAND
  • , Norbert TheobaldAffiliated withNorbert Theobald Federal Maritime and Hydrographic Agency Bernhard-Nochtstr. 78 20359 Hamburg DEUTSCHLAND

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Part I: Determination and identification of organic pollutants Part II: Results of the biotest battery and development of a biotest index


Preamble. This series of two papers presents the results of an interdisciplinary research project (ISIS) dealing with bioassay-directed fractionation of marine sediment extracts. Part I presents the extraction and fractionation procedure as well as the results of chemical analysis, including non-target analysis of sediments. Part II describes the results of the biotest battery in relation to chemicals possibly causing parts of the observed effects. A biotest index is used to compare the toxicities of the samples.

Goal, Scope and Background

Bioassay-directed fractionation (BDF) has become a valuable technique to investigate and characterise environmental samples with regard to toxicity. BDF was used as a tool to determine the ecotoxicological potential for marine sediments from the North Sea, the Baltic Sea, and the Skagerrak (samples taken far away from point sources). In order to look for the substances causing and contributing to the overall toxicity, the identification of priority compounds such as polycyclic aromatic hydrocarbons (PAH), polycylclic chlorinated biphenyls (PCB) and other organochlorines (OC), the quantitative determination of target substances of medium and high polarity, as well as a comprehensive, non-target screening were in the focus of this investigation: In this article the chemical results of the approach are described (Part I).


Sediment extracts were prepared by a sequential extraction of wet material with acetone and n-hexane. The extracts were subjected to a three step fractionation procedure by gel-permeation chromatography (GPC) and high pressure liquid chromatography (HPLC). Several compounds were quantified in the fractions: 16 PAHs, 21 other OCs, alkylphenols, nitroaromatics, synthetic musks, organo phosphorus compounds and brominated substances. Non-target analysis was performed using gas chromatography and mass spectrometry (GC/MS), and led to a long list of identified compounds in the samples.

Results and Discussion

Bioassay-directed fractionation was well suited to direct the chemical screening. The lipophilic contaminants PAHs and PCBs are still the predominant substances in the investigated marine sediments. Their concentrations were higher in sediment extracts from the Baltic Sea than in samples originating from the North Sea. Although lower concentration levels were found in North Sea samples, the contamination patterns of the North Sea samples were more complex, with a broader spectrum of biogenic and anthropogenic halogenated compounds. Especially some brominated indoles and phenols were detected in high concentrations in the North Sea sediments only. Generally, there were linear correlations between sediment characteristics, such as the total organic carbon (TOC) content and concentrations of some examined compounds. Compounds of biogenic origin such as brominated phenols and indoles can be assumed to contribute to toxicity in the polar HPLC fractions. Application of sediment quality guidelines demonstrates that the predicted effect levels were exceeded for some samples.


For the first time, a wide approach of chemical analysis and biological testing was applied to marine sediments of the North and Baltic Sea. The results of the chemical analyses of several lipophilic and polar target compounds, and a non-target screening in combination within the bioassay-directed fractionation approach delivered a complex data set about the contamination status of marine sediment samples. Concerning non-polar and some medium polar contaminants, a quite comprehensive description could be achieved, while less comprehensive data were obtained for more polar compounds.

Recommendation and Outlook

Toxicological effects were not restricted to industrial sites and harbours, but were found also in open sea areas. Anthropogenic as well as biogenic substances should be considered for marine sediment toxicity in future studies.

Baltic Sea bioassay-directed fractionation marine sediments non-target screening North Sea organic pollutants